气相色谱法测定柑桔中的硫线磷

报道了毛细管气相色谱法测定柑桔中残留硫线磷的方法。样品以乙腈提取,经石英毛细管气相色谱柱DB-1701分离,火焰光度检测器检测,外标法定量。方法的检出限为0.003mg/kg,相对标准偏差为3.47%—6.10%,加标回收率为80.37%—96.98%。     

基于内标法的钢铁中硫和磷激光诱导击穿光谱定量分析

利用激光诱导击穿光谱技术对铬钢样品中的硫、磷元素进行了定量分析.采用1 064nm Nd∶YAG固体激光器,在空气中激发样品,产生的光谱信号通过中阶梯光栅分光后进入EMCCD检测器,对波长在220~800nm范围的光谱信号进行检测.研究了光谱强度与延时时间以及激光能量之间的关系.在优化的实验参数下采用谱线强度比内标法定量分析三种铬钢样品中的硫、磷元素含量.实验结果表明,各元素定量结果的相对标准偏差最大值为2.6%,相对误差为-8.3%~12.5%.三种铬钢样品中硫含量分别为0.011%、0.0079%和0.0048%,磷含量分别为0.015%、0.014%和0.009%.激光诱导击穿光谱技术有望实现冶金工业的实时、在线和快速检测.     

高分辨连续光源原子吸收光谱法测定植物中的硫

硫元素在富燃的乙炔/空气火焰可形成CS双原子分子,在某些特定的波长下,这些CS分子吸收谱线具有原子吸收的轮廓和一定的吸收强度。文章主要研究利用高分辨连续光源原子吸收光谱法,通过测定硫元素在富燃-乙炔/空气火焰条件下形成的CS双原子分子的吸光度值,从而测定植物样品中的硫元素含量。实验对乙炔-空气比例和燃烧器高度等仪器条件进行了优化;实验研究了五种有机溶剂对CS分子吸收产生的影响情况、其他共存元素的光谱干扰和化学干扰以及不同的消解酸种类对测定结果的影响。在优化的条件下,硫在CS 257.961 nm的检出限为14 mg·L-1。通过对植物标准物质中硫含量的测定比对和精密度实验证明, 利用连续光源原子吸收光谱法,在富燃-乙炔/空气焰条件下以CS分子测定植物样品中的硫元素是一种简单、快速、有效的方法。     

SERS技术用于苹果表面有机磷农药残留的检测

传统农药残留检测方法比较繁琐、耗时、破坏样品,快速、无损、实时在线是农残检测的发展方向。本文利用表面增强拉曼光谱技术,以苹果为载体,有机磷农药甲拌磷和倍硫磷为研究对象,初步探讨了苹果表面甲拌磷和倍硫磷农药的快速无损检测方法。结果表明,运用表面增强拉曼光谱技术,可使两种有机磷农药的特征频率较易识别,并选取甲拌磷的728 cm-1和倍硫磷的1 512 cm-1 处的拉曼信号作为定量分析目标峰,采用内标法建立甲拌磷、倍硫磷的线性回归模型,可以作为定量分析甲拌磷、倍硫磷的参考依据。     

原子吸收光谱中火焰法和石墨炉法测定中草药中铜元素的比较研究

分别采用火焰原子吸收光谱法和石墨炉原子吸收光谱法测定5种中草药中铜元素的含量,比较两种方法测定铜元素的优劣。浓硝酸和双氧水微波消解处理样品,火焰原子吸收光谱法和石墨炉原子吸收光谱法分别测定其吸光度,校准曲线法计算元素含量。两种方法对于铜元素的检测有一定的差异,火焰法回收率在92.0%—102.0%之间,石墨炉法回收率在92.0%—110.0%。两种方法都能满足实验要求,但各有优点。     

气相色谱法测定土壤中15种农药的残留量

采用程序升温气相色谱法和氢火焰离子化检测器,对土壤中15种农药的残留量进行检测,该法简便、快速。     

微柱高效液相色谱与火焰光度检测器联用的初步研究

本文研究了常规高效液相色谱(HPLC)及微柱高效液相色谱(Micro-Column HPLC)与气相色谱火焰光度检测器(FPD)的联用技术及其应用.丁基锡等化合物经HPLC分离后,流出液通过FPD进行特效检测.接口采用将毛细管直接引入燃烧头的方式.文中对各有关参数进行了选择、优化和讨论, 对FPD作为HPLC的在线检测器的可能性作了初步探讨.     

整体柱毛细管电色谱法测定蔬菜中有机磷农药的含量

采用加压毛细管电色谱法,在整体柱上实现了马拉硫磷、二嗪农、甲基对硫磷、杀螟硫磷、倍硫磷、甲基毒死蜱和毒死蜱等 7 种有机磷类化合物的分离检测.整体固定相具有渗透性好,传质速度快等优点,7种物质10min内实现快速分离测定.在最佳电色谱条件下,马拉硫磷、二嗪农、甲基对硫磷、杀螟硫磷、倍硫磷、甲基毒死蜱和毒死蜱的线性范围分别为2-50μg/mL,2-50μg/mL,2-50μg/mL,2-50μg/mL,1.4-50μg/mL,2.5-50μg/mL,2.5-50μg/mL;相关系数r2为0.9925-0.9984;检测限(S/N=3)在0.3-1.5μg/mL之间.本法操作简单、快速,适合于蔬菜中有机磷农药残留的分析测定.     

有机磷农药残留的表面增强拉曼光谱快速检测

农药残留严重影响人类身体健康与生命安全,故亟需建立一种简单高效的农药残留快速检测方法。本文以金纳米溶胶作为表面增强拉曼光谱(SERS)的增强基底,结合便携式拉曼光谱仪,实现了倍硫磷与对硫磷等常用有机磷农药的多靶标同时检测。结果表明倍硫磷和对硫磷分别在1053 cm~(-1),1216 cm~(-1)和857 cm~(-1),1112 cm~(-1)处具有特征拉曼谱峰,且两者互不干扰。同时进一步研究表明,倍硫磷和对硫磷的浓度与其特征拉曼谱峰强度线性相关,故可实现定量检测,其中倍硫磷检测限可达0.01μg/mL对硫磷检测限可达0.025μg/mL。同时,该SERS方法可直接用于菠菜实际样品中多种农药残留的多靶标快速检测,检测限达到0.05μg/mL。该SERS方法具有方便、快速、灵敏度高、多靶标同时检测等优点,有望实现农药残留的现场快速检测。     

一种用于土壤非金属养分测试的光纤探头式分光光度计

针对测土配方施肥技术中要求快速、便捷、高效地进行土壤养分测试的需求,文章基于浸入式光纤探头、平场凹面全息光栅、二极管线阵检测器开发了一种光纤探头式分光光度计用于土壤养分中非金属元素的快速、准确测试。基于国家计量检定规程JJG 178—2007对紫外、可见、近红外分光光度计的性能检测方法测试的该仪器的波长最大允许误差与波长重复性、基线平直度、透射比最大允许误差与透射比重复性均达到了国标第Ⅲ级别标准,其最小光谱带宽、噪声与漂移、杂散光基本达到了国标第Ⅳ级别标准。基于该仪器测试的土壤硝态氮、铵态氮、有效磷、有效硫、有效硼、和有机质含量与基于商用的国产单光束和进口双光束分光光度计测试的结果呈极显著的线性相关关系,其回归方程的斜率接近于1,且对比数据之间无显著性差异。因此,该光纤探头式分光光度计可用于土壤非金属养分的快速、准确测试。     

Thermoelectric properties of Bi2Se3/Bi2Te3/Bi2Se3 and Sb2Te3/Bi2Te3/Sb2Te3 quantum well systems

In this work, we develop a theory of thermoelectric transport properties in two-dimensional semiconducting quantum well structures. Calculations are performed for n-type 0.1 wt.% CuBr-doped Bi₂Se₃/Bi₂Te₃/Bi₂Se₃ and p-type 3 wt.% Te-doped Sb₂Te₃/Bi₂Te₃/Sb₂Te₃ quantum well systems in the temperature range 50–600 K. It is found that reducing the well thickness has a pronounced effect on enhancing the thermoelectric figure of merit (ZT). For the n-type Bi₂Se₃/Bi₂Te₃/Bi₂Se₃ with 7 nm well width, the maximum value of ZT is estimated to be 0.97 at 350 K and for the p-type Sb₂Te₃/Bi₂Te₃/Sb₂Te₃ with well width 10 nm the highest value of the ZT is found to be 1.945 at 440 K. An explanation is provided for the resulting higher ZT value of the p-type system compared to the n-type system.     

La2/3Ca1/3MnO3/Eu2CuO4/La2/3Ca1/3MnO3磁性隧道结的制备与表征

采用磁控溅射,紫外线光刻和离子束刻蚀制备了La2/3Ca1/3MnO3lEu2CuO4/La2/3Ca1/3MnO3磁性隧道结.通过对获得的磁性隧道结的Ⅰ-Ⅴ特性测量,发现非线性的Ⅰ-Ⅴ特性,显示结样品的隧穿特性.有趣的是发现在电极材料La2/3Ca1/3MnO3的金属-绝缘体转变温度(Tp)以下,Ⅰ-Ⅴ曲线出现一个跳变.随着温度降低,开始出现跳变的临界电流增大,但是跳变都发生在同样的电压下～209mV.当电流增大或减小在跳变点附近出现回滞.这一跳变只发生在铁磁金属态,表明这是一个磁性相关联的效应,可能对应一种新的磁性开关过程.虽然,目前对这一现象背后的物理机理还不清楚,但是,这一现象有可能在未来自旋电子学器件方面具有潜在的应用价值.     

对靶溅射技术制备的La2/3Ca1/3MnO3/YBa2Cu4O8/La2/3Ca1/3MnO3薄膜中Tc的降低

本文用对靶溅射技术制备了La2/3Ca1/3MnO3/YBa2Cu4O8/La2/3Ca1/3MnO3薄膜.与YBCO单层薄膜相比,由于超导/铁磁系统中的磁性邻近效应,三层薄膜表现出较低的超导转变温度.薄膜的R～T测量曲线显示出超磁阻(CMR)效应和超导转变,预示着超导和铁磁特性共存于LCMO/YBCO/LCMO三文治结构.     

Physical properties of BaMg1/3Nb2/3O3-BaCo1/3Nb2/3O3 solid solutions

Structural, electric and magnetic properties of Ba₃Mg_1−xCo_xNb₂O₉ based dielectric ceramic compounds have been studied. The samples, prepared by a solid state reaction method, were characterised by X-ray powder diffraction (XRPD), electron microscopy (SEM), dielectric (ε(T)) and magnetic measurements (χ⁻¹(T)). The XRPD analyses showed that the crystal structure of these compounds does change by the increase of substitution degree, passing from a superstructure hexagonal-type, (no. 164), space group (SG) to a simple structure cubic-type, (no. 221), SG. However, the evolution of the elementary unit cell lattice parameter can be followed and it exhibit a linear increasing tendency with increase in the substitution, indicating the existence of a solid solution through out the investigated range of substitution (0-1). The microstructure analysis shows a variation in the grain size and also the porosity of the samples with the degree of substitution. The results are in good agreement with that of dielectric measurements, which also showed that the dielectric constant (ε) increases with the increase of cobalt content. The magnetic characterization of cobalt substituted samples showed an antiferromagnetic type super-exchange interaction between these magnetic ions. At the same time, the values of effective magnetic momentum (μ_eff) are close to the value that corresponds to Co²⁺ free ions. The study highlights the possibility of modelling these materials by substitutions, in order to improve properties of negative-positive-zero (NPO) type dielectric applications.     

La0.67Ca0.33MnO3薄膜皮秒光电效应

在1064 nm波长脉冲激光（脉宽25 ps）的照射下，钙钛矿氧化物薄膜La0.67Ca0.33MnO3/SrTiO3具有超快光电效应，对激光脉冲显示ps量级的响应时间，上升沿响应时间300 ps，半高宽700 ps，同时，对激光能量的响应灵敏度为500 mV/mJ。     

Giant dielectric relaxation in SrTiO3-SrMg1/3Nb2/3O3 and SrTiO3-SrSc1/2Ta1/2O3 solid solutions

Ceramic samples of (1−x)SrTiO₃-xSrMg_1/3Nb_2/3O₃ and (1−x)SrTiO₃-xSrSc_1/2Ta_1/2O₃ were prepared, and their dielectric properties were studied at x=0.005–0.15 and 0.01–0.1, respectively, at frequencies 10 Hz–1 MHz and at temperatures 4.2–350 K. A giant dielectric relaxation was observed in the temperature range 150–300 K, and not so strong but well-developed relaxation was found in the temperature range 20–90 K. The activation energy U and the relaxation time τ₀ were determined to be 0.21–0.3 eV and from 10⁻¹¹ to 10⁻¹² s for the high-temperature relaxation and 0.01–0.02 eV and 10⁻⁸–10⁻¹⁰ s for the low-temperature relaxation, respectively. The additional local charge compensation of the heterovalent impurities Mg²⁺ and Nb⁵⁺ (or Sc³⁺ and Ta⁵⁺) by free charge carriers or the host ion vacancies is suggested to be the underlying physical mechanism of the relaxation phenomena. On the basis of this mechanism, the Maxwell-Wagner model and the model of reorienting dipole centers Mg²⁺ (or Sc³⁺) associated with the oxygen vacancy are proposed to explain the high-temperature relaxation with some arguments in favor of the latter model. The polaron-like model with the Nb⁵⁺-Ti³⁺ center is suggested as the origin of the low-temperature relaxation. The reasons for the absence of ferroelectric phase transitions in the solid solutions under study are also discussed. From Fizika Tverdogo Tela, Vol. 44, No. 11, 2002, pp. 1948–1957. Original English Text Copyright ? 2002 by Lemanov, Sotnikov, Smirnova, Weihnacht. This article was submitted by the authors in English.     

Fluoride glasses in the InF3-GaF3-YF3-PbF2-CaF2-ZnF2 system

New glasses have been synthesized in a multicomponent system based on indium fluoride. Samples of a few mm in thickness were obtained. They are transparent and homogeneous. Main physical properties such as density, characteristic temperatures, density, thermal expansion and refractive index have been measured. The evolution versus composition is reported for samples with the formula: (35−x) InF₃-xGaF₃-10YF₃-25PbF₂-15CaF₂-15ZnF₂. T_g lies between 260 and 296 °C while melting starts around 480 °C. Glass samples are stable at room temperature. By comparison with other standard fluoride glasses, they exhibit higher refractive index and density.     

Luminescence properties of K1/2Bi1/2TiO3:Pr3+ and Na1/2Bi1/2TiO3:Pr3+

The luminescence properties of K(1/2)Bi(1/2)TiO(3):Pr(3+) and Na(1/2)Bi(1/2)TiO(3):Pr(3+) powders are investigated in the temperature range 10-600 K. The experimental data are interpreted on the basis of metal-to-metal charge transfer processes and by considering Bi(3+)-to-Pr(3+) sensitization effects.     

La2/3Ca1/3MnO3/Eu2CuO4/La2/3Ca1/3MnO3磁性隧道结的制备与表征

采用磁控溅射，紫外线光刻和离子束刻蚀制备了La_2/3Ca_1/3MnO₃/Eu₂CuO₄/La_2/3Ca_1/3MnO₃磁性隧道结.通过对获得的磁性隧道结的I-V特性测量，发现非线性的I-V特性，显示结样品的隧穿特性.有趣的是发现在电极材料La_2/3Ca_1/3MnO₃的金属-绝缘体转变温度(Tp)以下，I-V曲线出现一个跳变.随着温度降低，开始出现跳变的临界电流增大，但是跳变都发生在同样的电压下～209mV.当电流增大或减小在跳变点附近出现回滞.这一跳变只发生在铁磁金属态，表明这是一个磁性相关联的效应，可能对应一种新的磁性开关过程.虽然，目前对这一现象背后的物理机理还不清楚，但是，这一现象有可能在未来自旋电子学器件方面具有潜在的应用价值. 关键词： 庞磁电阻 磁性隧道结 开关效应     

Glass formation in the As2Se3-As2Te3-Sb2Te3 system

Chalcogenide glasses from the As₂Se₃-As₂Te₃-Sb₂Te₃ system were synthesized for the first time. The glass-forming region was determined by X-ray diffraction and electron microscopic analyses.The basic physicochemical parameters such as density (d), microhardness (HV) and temperatures of phase transformations (glass transition T_g, crystallization T_cr and melting T_m) were measured. Compactness and some thermomechanical characteristics such as volume (V_h) and formation energy (E_h) of micro-voids in the glassy network as well as the elasticity module (E) were calculated. The glass-forming ability was evaluated according to Hruby's criteria (K_G). The correlation between composition and properties of the (As₂Se₃)_x(As₂Te₃)_y(Sb₂Te₃)_z glasses was established and comprehensively discussed.